#------------------------------------------------------------------------------
#$Date: 2019-11-04 14:59:25 +0200 (Mon, 04 Nov 2019) $
#$Revision: 223081 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/03/45/4034595.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4034595
loop_
_publ_author_name
'Sampani, Stavroula I.'
'McGown, Andrew'
'Vargas, Alfredo'
'Abdul-Sada, Alaa'
'Tizzard, Graham J.'
'Coles, Simon J.'
'Spencer, John'
'Kostakis, George E.'
_publ_section_title
;
 Solvent-Free Synthesis and Key Intermediate Isolation in
 Ni₂Dy₂ Catalyst Development in the Domino
 Ring-Opening Electrocyclization Reaction of Furfural and Amines.
;
_journal_issue                   11
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6858
_journal_page_last               6867
_journal_paper_doi               10.1021/acs.joc.9b00608
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety
'C74 H86 Dy2 N10 Ni2 O18, 2(C F3 O3 S), 2(C3 H7 N O)'
_chemical_formula_sum            'C82 H100 Dy2 F6 N12 Ni2 O26 S2'
_chemical_formula_weight         2290.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-19
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.115(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7112(6)
_cell_length_b                   18.8566(7)
_cell_length_c                   15.7900(6)
_cell_measurement_reflns_used    6394
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.0600
_cell_measurement_theta_min      3.6490
_cell_volume                     4672.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -29.00  64.00   1.00    2.50    --   36.88 -77.00  60.00   93
  2  ω     47.00  84.00   1.00    7.50    --  107.00 -95.00  90.00   37
  3  ω     38.00  69.00   1.00    7.50    --  107.00 -95.00  30.00   31
  4  ω     39.00 116.00   1.00    7.50    --  107.00 -45.00 120.00   77
  5  ω     94.00 175.00   1.00    7.50    --  107.00  45.00 150.00   81
  6  ω    106.00 172.00   1.00    7.50    --  107.00  77.00-150.00   66
  7  ω     94.00 173.00   1.00    7.50    --  107.00  77.00-180.00   79
  8  ω     37.00  90.00   1.00    7.50    --  107.00-111.00-180.00   53
  9  ω     20.00 103.00   1.00    2.50    --   36.88  57.00-150.00   83
 10  ω   -109.00 -57.00   1.00    2.50    --  -36.88-178.00-120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0331033000
_diffrn_orient_matrix_UB_12      0.0695269000
_diffrn_orient_matrix_UB_13      0.0512064000
_diffrn_orient_matrix_UB_21      0.0919553000
_diffrn_orient_matrix_UB_22      -0.0206422000
_diffrn_orient_matrix_UB_23      0.0089055000
_diffrn_orient_matrix_UB_31      -0.0110648000
_diffrn_orient_matrix_UB_32      0.0375580000
_diffrn_orient_matrix_UB_33      -0.0897773000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14643
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.857
_diffrn_reflns_theta_min         4.690
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.178
_refine_diff_density_min         -2.231
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         8755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0911P)²+2.4796P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7511
_reflns_number_total             8755
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jo9b00608_si_001.cif
_cod_data_source_block           sis541b
_cod_database_code               4034595
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C176 H212 Dy4 N24 Ni4 O52 S2 F2'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 98.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C19(H19), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C32(H32), C35(H35), C38(H38)
;
_olex2_date_sample_data_collection 2018-02-19
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.585
_oxdiff_exptl_absorpt_empirical_full_min 0.447
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Dy1 Dy 0.32140(2) 0.48592(2) 0.35080(2) 0.02381(12) Uani 1 1 d .
Ni1 Ni 0.45872(5) 0.47796(4) 0.57301(6) 0.0222(2) Uani 1 1 d .
O1 O 0.3261(2) 0.3538(2) 0.3215(2) 0.0292(8) Uani 1 1 d .
O2 O 0.3784(2) 0.41611(17) 0.4751(2) 0.0222(7) Uani 1 1 d .
O3 O 0.5523(2) 0.52223(19) 0.6834(2) 0.0242(7) Uani 1 1 d .
O4 O 0.1877(4) 0.4359(3) 0.0476(3) 0.0529(13) Uani 1 1 d .
O5 O 0.2576(3) 0.4927(2) 0.2059(3) 0.0327(8) Uani 1 1 d .
O6 O 0.4344(2) 0.54855(17) 0.4654(2) 0.0206(6) Uani 1 1 d .
O7 O 0.1858(2) 0.4304(2) 0.3297(3) 0.0374(9) Uani 1 1 d .
O8 O 0.2433(2) 0.5560(2) 0.4189(3) 0.0326(8) Uani 1 1 d .
O9 O 0.3678(2) 0.5302(2) 0.6122(3) 0.0302(8) Uani 1 1 d .
N1 N 0.4642(3) 0.4014(2) 0.6629(3) 0.0261(9) Uani 1 1 d .
N2 N 0.3353(3) 0.6104(2) 0.3104(3) 0.0254(9) Uani 1 1 d .
N3 N 0.0639(4) 0.3731(4) 0.2525(5) 0.0592(18) Uani 1 1 d .
N4 N 0.1697(3) 0.5910(3) 0.5070(3) 0.0363(11) Uani 1 1 d .
N5 N 0.3232(3) 0.5504(3) 0.7289(3) 0.0437(13) Uani 1 1 d .
C1 C 0.2921(5) 0.3218(3) 0.2341(4) 0.0486(17) Uani 1 1 d .
H1A H 0.2827 0.3584 0.1876 0.073 Uiso 1 1 calc R
H1B H 0.3325 0.2865 0.2272 0.073 Uiso 1 1 calc R
H1C H 0.2379 0.2986 0.2277 0.073 Uiso 1 1 calc R
C2 C 0.3434(3) 0.3102(3) 0.3953(4) 0.0284(11) Uani 1 1 d .
C3 C 0.3348(4) 0.2359(3) 0.3914(4) 0.0320(12) Uani 1 1 d .
H3 H 0.3123 0.2125 0.3348 0.038 Uiso 1 1 calc R
C4 C 0.3595(4) 0.1969(3) 0.4715(4) 0.0402(13) Uani 1 1 d .
H4 H 0.3532 0.1468 0.4698 0.048 Uiso 1 1 calc R
C5 C 0.3929(4) 0.2314(3) 0.5527(4) 0.0357(12) Uani 1 1 d .
H5 H 0.4103 0.2042 0.6066 0.043 Uiso 1 1 calc R
C6 C 0.4022(3) 0.3057(3) 0.5590(4) 0.0284(11) Uani 1 1 d .
C7 C 0.3751(3) 0.3462(3) 0.4789(4) 0.0272(11) Uani 1 1 d .
C8 C 0.4406(3) 0.3361(3) 0.6475(4) 0.0291(11) Uani 1 1 d .
H8 H 0.4490 0.3060 0.6981 0.035 Uiso 1 1 calc R
C9 C 0.4969(3) 0.4301(3) 0.7509(4) 0.0283(11) Uani 1 1 d .
C10 C 0.4858(3) 0.4013(3) 0.8275(4) 0.0325(12) Uani 1 1 d .
H10 H 0.4551 0.3582 0.8227 0.039 Uiso 1 1 calc R
C11 C 0.5190(4) 0.4347(3) 0.9103(4) 0.0353(12) Uani 1 1 d .
H11 H 0.5120 0.4144 0.9624 0.042 Uiso 1 1 calc R
C12 C 0.5622(4) 0.4974(4) 0.9162(4) 0.0369(13) Uani 1 1 d .
H12 H 0.5849 0.5203 0.9731 0.044 Uiso 1 1 calc R
C13 C 0.5736(4) 0.5285(3) 0.8414(4) 0.0321(12) Uani 1 1 d .
H13 H 0.6029 0.5724 0.8473 0.039 Uiso 1 1 calc R
C14 C 0.5415(3) 0.4947(3) 0.7567(4) 0.0247(10) Uani 1 1 d .
C15 C 0.1611(6) 0.3995(5) -0.0354(5) 0.062(2) Uani 1 1 d .
H15A H 0.1488 0.3500 -0.0256 0.093 Uiso 1 1 calc R
H15B H 0.1096 0.4219 -0.0768 0.093 Uiso 1 1 calc R
H15C H 0.2064 0.4012 -0.0616 0.093 Uiso 1 1 calc R
C16 C 0.2080(4) 0.5061(3) 0.0484(4) 0.0355(12) Uani 1 1 d .
C17 C 0.1961(4) 0.5477(4) -0.0268(4) 0.0409(14) Uani 1 1 d .
H17 H 0.1685 0.5284 -0.0852 0.049 Uiso 1 1 calc R
C18 C 0.2241(4) 0.6177(4) -0.0180(4) 0.0398(14) Uani 1 1 d .
H18 H 0.2159 0.6459 -0.0701 0.048 Uiso 1 1 calc R
C19 C 0.2639(4) 0.6460(3) 0.0674(4) 0.0363(13) Uani 1 1 d .
H19 H 0.2831 0.6938 0.0732 0.044 Uiso 1 1 calc R
C20 C 0.2764(3) 0.6049(3) 0.1455(4) 0.0293(11) Uani 1 1 d .
C21 C 0.2475(3) 0.5342(4) 0.1369(4) 0.0337(12) Uani 1 1 d .
C22 C 0.3180(3) 0.6392(3) 0.2310(4) 0.0260(10) Uani 1 1 d .
H22 H 0.3344 0.6873 0.2293 0.031 Uiso 1 1 calc R
C23 C 0.3721(3) 0.6534(3) 0.3887(4) 0.0255(10) Uani 1 1 d .
C24 C 0.3576(4) 0.7275(3) 0.3902(4) 0.0300(11) Uani 1 1 d .
H24 H 0.3247 0.7512 0.3363 0.036 Uiso 1 1 calc R
C25 C 0.3907(3) 0.7655(3) 0.4692(4) 0.0338(12) Uani 1 1 d .
H25 H 0.3816 0.8152 0.4696 0.041 Uiso 1 1 calc R
C26 C 0.4377(4) 0.7306(3) 0.5485(4) 0.0315(11) Uani 1 1 d .
H26 H 0.4604 0.7566 0.6030 0.038 Uiso 1 1 calc R
C27 C 0.4516(3) 0.6575(3) 0.5482(3) 0.0249(10) Uani 1 1 d .
H27 H 0.4831 0.6339 0.6026 0.030 Uiso 1 1 calc R
C28 C 0.4195(3) 0.6195(3) 0.4688(3) 0.0237(10) Uani 1 1 d .
C29 C 0.1312(4) 0.4088(4) 0.2574(5) 0.0479(16) Uani 1 1 d .
H29 H 0.1402 0.4196 0.2025 0.058 Uiso 1 1 calc R
C30 C 0.0537(10) 0.3465(11) 0.3328(9) 0.187(11) Uani 1 1 d .
H30A H -0.0005 0.3208 0.3172 0.281 Uiso 1 1 calc R
H30B H 0.1008 0.3143 0.3633 0.281 Uiso 1 1 calc R
H30C H 0.0536 0.3861 0.3729 0.281 Uiso 1 1 calc R
C31 C 0.0056(6) 0.3484(6) 0.1660(7) 0.090(4) Uani 1 1 d .
H31A H -0.0415 0.3224 0.1753 0.135 Uiso 1 1 calc R
H31B H -0.0170 0.3891 0.1266 0.135 Uiso 1 1 calc R
H31C H 0.0360 0.3170 0.1380 0.135 Uiso 1 1 calc R
C32 C 0.1972(3) 0.5421(3) 0.4634(4) 0.0317(12) Uani 1 1 d .
H32 H 0.1808 0.4942 0.4665 0.038 Uiso 1 1 calc R
C33 C 0.1962(5) 0.6635(4) 0.5085(5) 0.0502(17) Uani 1 1 d .
H33A H 0.1697 0.6920 0.5436 0.075 Uiso 1 1 calc R
H33B H 0.2584 0.6664 0.5362 0.075 Uiso 1 1 calc R
H33C H 0.1787 0.6818 0.4467 0.075 Uiso 1 1 calc R
C34 C 0.1119(4) 0.5736(4) 0.5552(5) 0.0487(16) Uani 1 1 d .
H34A H 0.0989 0.6166 0.5828 0.073 Uiso 1 1 calc R
H34B H 0.0590 0.5538 0.5128 0.073 Uiso 1 1 calc R
H34C H 0.1388 0.5386 0.6022 0.073 Uiso 1 1 calc R
C35 C 0.3341(4) 0.5097(3) 0.6662(4) 0.0322(12) Uani 1 1 d .
H35 H 0.3150 0.4619 0.6623 0.039 Uiso 1 1 calc R
C36 C 0.3541(6) 0.6227(5) 0.7409(6) 0.070(2) Uani 1 1 d .
H36A H 0.3403 0.6448 0.7904 0.105 Uiso 1 1 calc R
H36B H 0.4160 0.6229 0.7552 0.105 Uiso 1 1 calc R
H36C H 0.3268 0.6495 0.6852 0.105 Uiso 1 1 calc R
C37 C 0.2842(7) 0.5232(6) 0.7917(6) 0.079(3) Uani 1 1 d .
H37A H 0.2816 0.5611 0.8332 0.118 Uiso 1 1 calc R
H37B H 0.2265 0.5065 0.7582 0.118 Uiso 1 1 calc R
H37C H 0.3184 0.4838 0.8262 0.118 Uiso 1 1 calc R
S1 S 0.15737(12) 0.34048(10) 0.61764(13) 0.0527(4) Uani 1 1 d .
F1 F 0.1019(5) 0.4239(4) 0.7183(5) 0.106(2) Uani 1 1 d .
F2 F 0.0102(3) 0.3475(4) 0.6427(4) 0.100(2) Uani 1 1 d .
F3 F 0.1131(4) 0.3149(4) 0.7575(4) 0.101(2) Uani 1 1 d .
O10 O 0.1297(5) 0.3947(4) 0.5503(4) 0.081(2) Uani 1 1 d .
O11 O 0.1351(4) 0.2688(3) 0.5862(4) 0.0749(18) Uani 1 1 d .
O12 O 0.2429(4) 0.3495(3) 0.6808(4) 0.0637(14) Uani 1 1 d .
C41 C 0.0949(6) 0.3577(6) 0.6871(6) 0.065(2) Uani 1 1 d .
O13 O 0.1647(4) 0.7870(4) 0.2262(5) 0.0753(18) Uani 1 1 d .
N6 N 0.0963(4) 0.6810(4) 0.1823(4) 0.0555(16) Uani 1 1 d .
C38 C 0.1469(5) 0.7260(6) 0.2410(6) 0.064(2) Uani 1 1 d .
H38 H 0.1723 0.7093 0.3011 0.077 Uiso 1 1 calc R
C39 C 0.0855(6) 0.6099(5) 0.2057(7) 0.071(2) Uani 1 1 d .
H39A H 0.0458 0.5855 0.1533 0.106 Uiso 1 1 calc R
H39B H 0.1406 0.5855 0.2250 0.106 Uiso 1 1 calc R
H39C H 0.0626 0.6096 0.2551 0.106 Uiso 1 1 calc R
C40 C 0.0576(6) 0.7009(6) 0.0872(6) 0.077(3) Uani 1 1 d .
H40A H 0.0224 0.6617 0.0536 0.115 Uiso 1 1 calc R
H40B H 0.0220 0.7431 0.0821 0.115 Uiso 1 1 calc R
H40C H 0.1025 0.7112 0.0623 0.115 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Dy1 Ni1 95.18(8) . .
O2 Dy1 Ni1 33.98(8) . .
O2 Dy1 O1 63.93(12) . .
O2 Dy1 O3 90.98(12) . 3_666
O2 Dy1 O6 69.62(11) . .
O2 Dy1 O7 87.89(14) . .
O2 Dy1 O8 93.68(13) . .
O2 Dy1 N2 136.34(13) . .
O3 Dy1 Ni1 84.02(9) 3_666 .
O3 Dy1 O1 78.92(12) 3_666 .
O3 Dy1 O6 70.96(12) 3_666 .
O3 Dy1 O7 144.39(13) 3_666 .
O3 Dy1 O8 145.09(13) 3_666 .
O3 Dy1 N2 80.27(13) 3_666 .
O5 Dy1 Ni1 169.12(11) . .
O5 Dy1 O1 84.32(14) . .
O5 Dy1 O2 148.13(13) . .
O5 Dy1 O3 85.22(14) . 3_666
O5 Dy1 O6 137.03(13) . .
O5 Dy1 O7 77.45(15) . .
O5 Dy1 O8 107.38(15) . .
O5 Dy1 N2 74.15(15) . .
O6 Dy1 Ni1 36.21(8) . .
O6 Dy1 O1 123.25(11) . .
O6 Dy1 N2 67.08(12) . .
O7 Dy1 Ni1 112.55(11) . .
O7 Dy1 O1 68.68(14) . .
O7 Dy1 O6 140.10(12) . .
O7 Dy1 N2 123.04(15) . .
O8 Dy1 Ni1 80.85(10) . .
O8 Dy1 O1 133.53(13) . .
O8 Dy1 O6 78.37(12) . .
O8 Dy1 O7 70.42(14) . .
O8 Dy1 N2 72.60(14) . .
N2 Dy1 Ni1 102.37(10) . .
N2 Dy1 O1 151.11(14) . .
O2 Ni1 Dy1 38.88(9) . .
O2 Ni1 O3 168.62(14) . .
O2 Ni1 O6 92.72(14) . 3_666
O2 Ni1 O6 81.57(13) . .
O2 Ni1 O9 98.04(16) . .
O3 Ni1 Dy1 151.22(10) . .
O3 Ni1 O6 82.55(14) . 3_666
O3 Ni1 O6 107.89(14) . .
O3 Ni1 O9 88.63(15) . .
O6 Ni1 Dy1 92.87(9) 3_666 .
O6 Ni1 Dy1 43.39(9) . .
O6 Ni1 O6 82.29(14) . 3_666
O9 Ni1 Dy1 89.05(11) . .
O9 Ni1 O6 165.00(15) . 3_666
O9 Ni1 O6 88.97(14) . .
N1 Ni1 Dy1 126.87(13) . .
N1 Ni1 O2 89.02(16) . .
N1 Ni1 O3 81.79(17) . .
N1 Ni1 O6 170.16(16) . .
N1 Ni1 O6 101.14(15) . 3_666
N1 Ni1 O9 89.50(17) . .
C1 O1 Dy1 124.1(3) . .
C2 O1 Dy1 116.3(3) . .
C2 O1 C1 117.7(4) . .
Ni1 O2 Dy1 107.14(14) . .
C7 O2 Dy1 127.1(3) . .
C7 O2 Ni1 124.4(3) . .
Ni1 O3 Dy1 104.89(15) . 3_666
C14 O3 Dy1 124.8(3) . 3_666
C14 O3 Ni1 106.5(3) . .
C16 O4 C15 118.7(6) . .
C21 O5 Dy1 142.3(4) . .
Ni1 O6 Dy1 100.78(13) 3_666 .
Ni1 O6 Dy1 100.41(13) . .
Ni1 O6 Ni1 97.71(14) . 3_666
C28 O6 Dy1 113.6(3) . .
C28 O6 Ni1 115.0(3) . 3_666
C28 O6 Ni1 125.5(3) . .
C29 O7 Dy1 128.1(4) . .
C32 O8 Dy1 133.7(4) . .
C35 O9 Ni1 127.7(4) . .
C8 N1 Ni1 128.1(4) . .
C8 N1 C9 122.7(5) . .
C9 N1 Ni1 109.2(3) . .
C22 N2 Dy1 129.5(4) . .
C22 N2 C23 118.9(4) . .
C23 N2 Dy1 111.6(3) . .
C29 N3 C30 120.0(8) . .
C29 N3 C31 120.8(8) . .
C30 N3 C31 118.3(8) . .
C32 N4 C33 120.8(5) . .
C32 N4 C34 121.7(6) . .
C33 N4 C34 117.6(6) . .
C35 N5 C36 120.9(6) . .
C35 N5 C37 121.2(7) . .
C36 N5 C37 117.7(7) . .
O1 C1 H1A 109.5 . .
O1 C1 H1B 109.5 . .
O1 C1 H1C 109.5 . .
H1A C1 H1B 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
O1 C2 C3 124.7(5) . .
O1 C2 C7 114.1(5) . .
C3 C2 C7 121.2(5) . .
C2 C3 H3 120.3 . .
C4 C3 C2 119.3(5) . .
C4 C3 H3 120.3 . .
C3 C4 H4 120.2 . .
C5 C4 C3 119.6(5) . .
C5 C4 H4 120.2 . .
C4 C5 H5 118.8 . .
C4 C5 C6 122.5(6) . .
C6 C5 H5 118.8 . .
C5 C6 C7 118.7(5) . .
C5 C6 C8 117.8(5) . .
C7 C6 C8 123.5(5) . .
O2 C7 C2 116.3(5) . .
O2 C7 C6 125.0(5) . .
C6 C7 C2 118.6(5) . .
N1 C8 C6 124.6(5) . .
N1 C8 H8 117.7 . .
C6 C8 H8 117.7 . .
N1 C9 C14 114.2(5) . .
C10 C9 N1 125.6(5) . .
C10 C9 C14 120.1(5) . .
C9 C10 H10 119.6 . .
C11 C10 C9 120.9(6) . .
C11 C10 H10 119.6 . .
C10 C11 H11 120.5 . .
C12 C11 C10 119.1(5) . .
C12 C11 H11 120.5 . .
C11 C12 H12 119.0 . .
C11 C12 C13 122.0(6) . .
C13 C12 H12 119.0 . .
C12 C13 H13 120.1 . .
C12 C13 C14 119.7(6) . .
C14 C13 H13 120.1 . .
O3 C14 C9 120.2(5) . .
O3 C14 C13 121.7(5) . .
C13 C14 C9 118.1(5) . .
O4 C15 H15A 109.5 . .
O4 C15 H15B 109.5 . .
O4 C15 H15C 109.5 . .
H15A C15 H15B 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
O4 C16 C17 125.6(6) . .
O4 C16 C21 113.6(6) . .
C17 C16 C21 120.8(6) . .
C16 C17 H17 119.7 . .
C16 C17 C18 120.7(6) . .
C18 C17 H17 119.7 . .
C17 C18 H18 120.2 . .
C19 C18 C17 119.7(6) . .
C19 C18 H18 120.2 . .
C18 C19 H19 119.5 . .
C18 C19 C20 120.9(6) . .
C20 C19 H19 119.5 . .
C19 C20 C22 116.7(5) . .
C21 C20 C19 119.6(5) . .
C21 C20 C22 123.6(5) . .
O5 C21 C16 118.6(6) . .
O5 C21 C20 123.1(5) . .
C20 C21 C16 118.3(6) . .
N2 C22 C20 126.1(5) . .
N2 C22 H22 117.0 . .
C20 C22 H22 117.0 . .
C24 C23 N2 123.2(5) . .
C28 C23 N2 117.8(4) . .
C28 C23 C24 118.8(5) . .
C23 C24 H24 119.7 . .
C25 C24 C23 120.5(5) . .
C25 C24 H24 119.7 . .
C24 C25 H25 120.2 . .
C24 C25 C26 119.7(5) . .
C26 C25 H25 120.2 . .
C25 C26 H26 119.8 . .
C25 C26 C27 120.4(5) . .
C27 C26 H26 119.8 . .
C26 C27 H27 120.0 . .
C28 C27 C26 120.0(5) . .
C28 C27 H27 120.0 . .
O6 C28 C23 117.8(4) . .
O6 C28 C27 121.6(4) . .
C27 C28 C23 120.6(5) . .
O7 C29 N3 124.5(7) . .
O7 C29 H29 117.8 . .
N3 C29 H29 117.8 . .
N3 C30 H30A 109.5 . .
N3 C30 H30B 109.5 . .
N3 C30 H30C 109.5 . .
H30A C30 H30B 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
N3 C31 H31A 109.5 . .
N3 C31 H31B 109.5 . .
N3 C31 H31C 109.5 . .
H31A C31 H31B 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
O8 C32 N4 122.9(6) . .
O8 C32 H32 118.5 . .
N4 C32 H32 118.5 . .
N4 C33 H33A 109.5 . .
N4 C33 H33B 109.5 . .
N4 C33 H33C 109.5 . .
H33A C33 H33B 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
N4 C34 H34A 109.5 . .
N4 C34 H34B 109.5 . .
N4 C34 H34C 109.5 . .
H34A C34 H34B 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
O9 C35 N5 123.4(6) . .
O9 C35 H35 118.3 . .
N5 C35 H35 118.3 . .
N5 C36 H36A 109.5 . .
N5 C36 H36B 109.5 . .
N5 C36 H36C 109.5 . .
H36A C36 H36B 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
N5 C37 H37A 109.5 . .
N5 C37 H37B 109.5 . .
N5 C37 H37C 109.5 . .
H37A C37 H37B 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
O10 S1 O11 115.7(4) . .
O10 S1 O12 114.7(4) . .
O10 S1 C41 102.6(4) . .
O11 S1 C41 104.2(5) . .
O12 S1 O11 115.1(4) . .
O12 S1 C41 101.7(4) . .
F1 C41 S1 113.7(7) . .
F1 C41 F2 105.5(8) . .
F2 C41 S1 112.4(6) . .
F3 C41 S1 113.0(7) . .
F3 C41 F1 107.2(8) . .
F3 C41 F2 104.2(8) . .
C38 N6 C39 122.1(8) . .
C38 N6 C40 120.2(8) . .
C39 N6 C40 117.3(8) . .
O13 C38 N6 127.2(8) . .
O13 C38 H38 116.4 . .
N6 C38 H38 116.4 . .
N6 C39 H39A 109.5 . .
N6 C39 H39B 109.5 . .
N6 C39 H39C 109.5 . .
H39A C39 H39B 109.5 . .
H39A C39 H39C 109.5 . .
H39B C39 H39C 109.5 . .
N6 C40 H40A 109.5 . .
N6 C40 H40B 109.5 . .
N6 C40 H40C 109.5 . .
H40A C40 H40B 109.5 . .
H40A C40 H40C 109.5 . .
H40B C40 H40C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 Ni1 3.4730(9) .
Dy1 O1 2.541(4) .
Dy1 O2 2.281(3) .
Dy1 O3 2.357(4) 3_666
Dy1 O5 2.170(4) .
Dy1 O6 2.425(3) .
Dy1 O7 2.413(4) .
Dy1 O8 2.360(4) .
Dy1 N2 2.464(4) .
Ni1 O2 2.031(3) .
Ni1 O3 2.075(4) .
Ni1 O6 2.134(3) 3_666
Ni1 O6 2.086(3) .
Ni1 O9 2.076(4) .
Ni1 N1 2.005(4) .
O1 C1 1.433(7) .
O1 C2 1.372(7) .
O2 C7 1.322(7) .
O3 Dy1 2.357(4) 3_666
O3 C14 1.337(7) .
O4 C15 1.410(8) .
O4 C16 1.364(8) .
O5 C21 1.305(7) .
O6 Ni1 2.134(3) 3_666
O6 C28 1.366(6) .
O7 C29 1.260(8) .
O8 C32 1.236(7) .
O9 C35 1.236(7) .
N1 C8 1.290(7) .
N1 C9 1.414(7) .
N2 C22 1.305(7) .
N2 C23 1.427(7) .
N3 C29 1.291(9) .
N3 C30 1.427(15) .
N3 C31 1.455(10) .
N4 C32 1.325(8) .
N4 C33 1.435(9) .
N4 C34 1.458(8) .
N5 C35 1.313(8) .
N5 C36 1.448(11) .
N5 C37 1.455(10) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.409(7) .
C2 C7 1.414(8) .
C3 H3 0.9500 .
C3 C4 1.398(9) .
C4 H4 0.9500 .
C4 C5 1.373(9) .
C5 H5 0.9500 .
C5 C6 1.409(8) .
C6 C7 1.413(7) .
C6 C8 1.441(8) .
C8 H8 0.9500 .
C9 C10 1.395(8) .
C9 C14 1.415(8) .
C10 H10 0.9500 .
C10 C11 1.384(8) .
C11 H11 0.9500 .
C11 C12 1.372(10) .
C12 H12 0.9500 .
C12 C13 1.388(9) .
C13 H13 0.9500 .
C13 C14 1.411(8) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C17 1.380(9) .
C16 C21 1.427(8) .
C17 H17 0.9500 .
C17 C18 1.390(10) .
C18 H18 0.9500 .
C18 C19 1.388(9) .
C19 H19 0.9500 .
C19 C20 1.411(8) .
C20 C21 1.407(9) .
C20 C22 1.443(7) .
C22 H22 0.9500 .
C23 C24 1.421(7) .
C23 C28 1.395(7) .
C24 H24 0.9500 .
C24 C25 1.379(8) .
C25 H25 0.9500 .
C25 C26 1.392(8) .
C26 H26 0.9500 .
C26 C27 1.399(8) .
C27 H27 0.9500 .
C27 C28 1.382(7) .
C29 H29 0.9500 .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 H32 0.9500 .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
C35 H35 0.9500 .
C36 H36A 0.9800 .
C36 H36B 0.9800 .
C36 H36C 0.9800 .
C37 H37A 0.9800 .
C37 H37B 0.9800 .
C37 H37C 0.9800 .
S1 O10 1.433(6) .
S1 O11 1.445(7) .
S1 O12 1.445(6) .
S1 C41 1.785(9) .
F1 C41 1.332(12) .
F2 C41 1.359(10) .
F3 C41 1.322(10) .
O13 C38 1.230(11) .
N6 C38 1.324(12) .
N6 C39 1.419(11) .
N6 C40 1.465(10) .
C38 H38 0.9500 .
C39 H39A 0.9800 .
C39 H39B 0.9800 .
C39 H39C 0.9800 .
C40 H40A 0.9800 .
C40 H40B 0.9800 .
C40 H40C 0.9800 .
